Solid State NMR techniques will be developed and applied to the investigation of structural and dynamical properties of peptides and proteins. Nitrogen-14 single crystal NMR will be developed and used to determine structures of polypeptides and 13C and 15N magic angle sample spinning (MASS) spectra will be used for the first direct comparison of solution and solid state structure of peptides and proteins. Moreover, MASS technique will permit observation of the rate and anisotropy of side chain dynamics in these molecules. Near neighbor NMR will be developed and employed to study structure of metal binding and spin labeled sites. Finally, several techniques--including dynamic nuclear polarization, off resonance decoupling, and solid state versions of INEPT--are suggested for enhancing the capabilities of these methods.